CN118000417A

CN118000417A - Compound microcapsule powder and preparation method and application thereof

Info

Publication number: CN118000417A
Application number: CN202410323502.1A
Authority: CN
Inventors: 李倩; 宿惊涛; 张妍; 范超; 张鑫玉; 吴文忠
Original assignee: Innobio Corp ltd
Current assignee: Innobio Corp ltd
Priority date: 2024-03-20
Filing date: 2024-03-20
Publication date: 2024-05-10

Abstract

The invention provides a compound microcapsule powder and a preparation method and application thereof, wherein the compound microcapsule powder comprises 10-20 parts of astaxanthin microcapsule powder, 100-200 parts of hydrolyzed collagen and 2-7 parts of vitamin C microcapsule powder; the astaxanthin microcapsule powder is prepared by the following method, which comprises the following steps: (1) Pretreating astaxanthin oleoresin to obtain astaxanthin pretreatment; (2) And dissolving the astaxanthin pretreatment in embedding mixed solution, pre-emulsifying and homogenizing to obtain emulsion, heating, stirring and spray-drying the emulsion to obtain the astaxanthin microcapsule powder. The composite microcapsule powder provided by the invention has high stability, high bioavailability and good antioxidation effect, overcomes the problems of easy deterioration and low bioavailability of astaxanthin raw materials in the prior practical application, and also overcomes the problems of easy color changing and caking of vitamin C and collagen compounding.

Description

Compound microcapsule powder and preparation method and application thereof

Technical Field

The invention belongs to the technical field of health care and beauty treatment, and particularly relates to compound microcapsule powder and a preparation method and application thereof.

Background

Astaxanthin is formed by connecting 4 isoprene double bonds end to end, has 11 conjugated double bonds in total, has a molecular formula of C ₄₀H₅₂O₄ and a relative molecular weight of 596.86, and is a ketone carotenoid. Astaxanthin is fat-soluble, insoluble in water, and has extremely strong pigmentation ability, and can be used as a functional pigment as a colorant. Meanwhile, astaxanthin has very strong antioxidation and anti-photosensitive effects, is used as a substance with the strongest antioxidation capability of the natural sources found at present, and has unique effects in the aspects of delaying aging, enhancing resistance and preventing and treating Alzheimer's disease and cancer.

However, astaxanthin is limited to capsules and powders in its application form due to its extremely poor water solubility. In addition, due to the unique structure of astaxanthin, the astaxanthin is unstable in property and easy to isomerize and degrade, so that the application of astaxanthin is limited to a large extent.

Collagen is a structural material, and 70% -85% of the dermal tissue of human skin is collagen. The content is highest at 18 years old, and later begins to slowly run off until 40 years old, and only half of the content remains. The main function of the collagen is that the whole epidermal tissue is supported like a bracket or a spring, so that the skin looks plump, the collagen is absent in the skin, the collagen fiber is crosslinked and solidified, the intercellular mucopolysaccharide is reduced, the skin loses elasticity and thins, ages, and the problems of color spots, large pores, wrinkles and the like appear. More and more people hope to keep the skin in a young state by supplementing collagen, but most of the collagen sold in the market is macromolecular substances, so that the collagen is difficult to absorb in human bodies to achieve the effect, has a certain bitter taste, and is difficult to drink directly as a product.

Vitamin C is a common vitamin, has oxidation resistance, and can prevent free radical injury to human body. Meanwhile, the synthesis of collagen needs to participate in vitamin C, so that under the condition of VC deficiency, collagen cannot be normally synthesized. However, collagen has the property of protein, and can cause the problems of flocculation, caking, color change and the like under the acidic condition. This greatly restricts the use of ascorbic acid and collagen.

CN111213807a discloses an astaxanthin collagen liquid drink and a preparation method thereof, wherein the astaxanthin collagen liquid drink comprises the following components in parts by mass: 0.01-0.1 part of astaxanthin oleoresin, 0.1-10 parts of embedding wall material, 0.05-1.0 part of filling material, 1-20 parts of collagen, 0.015-0.3 part of emulsifier, 0.001-0.02 part of auxiliary emulsifier and 68-99 parts of diluent medium water; the problems of collagen absorption are solved, the particle size of the astaxanthin collagen liquid beverage is reduced to the nanometer level by the combined use of the wall material, the filling material and the emulsifying agent, the astaxanthin collagen liquid beverage is uniform and stable within the shelf life, the bioavailability and the improvement effect on the skin are improved, and the astaxanthin collagen liquid beverage can also be directly seasoned and is suitable for liquid products with different pH conditions.

CN112869150a discloses an astaxanthin composition, a preparation method, a preparation and application thereof, wherein the astaxanthin composition comprises astaxanthin, bonito elastin peptide, fish collagen peptide, natural vitamin C and hyaluronic acid. The astaxanthin composition is applied to the preparation of products for moisturizing skin, resisting wrinkle, tightening skin, brightening skin, resisting freckle, improving skin texture, improving rough skin caused by long-wave ultraviolet rays in UVB-UVA, reducing skin inflammation, resisting oxidation and beautifying and resisting aging.

CN106798330a discloses an astaxanthin collagen peptide powder and a preparation method thereof, wherein astaxanthin microcapsule powder and pure fish collagen powder are taken according to the weight ratio of 1:832; uniformly mixing at 16-20deg.C and humidity of 30-35% RH to obtain astaxanthin collagen peptide powder; and after weighing, the astaxanthin collagen peptide powder is vacuumized and packaged by a packaging machine, wherein each bag of astaxanthin collagen peptide powder is 5 g, and when the astaxanthin collagen peptide powder is taken, the packaging bag is torn open to be directly taken with warm boiled water, and the astaxanthin and the collagen are combined, so that the astaxanthin and the collagen are high in nutritive value and convenient to eat.

In the prior art, astaxanthin and collagen are compounded to form a liquid drink, but the product has poor effect and low bioavailability, and simultaneously, the color change phenomenon can occur when the collagen and the vitamin C are mixed. These problems have greatly limited the administration of oral cosmetic astaxanthin, ascorbic acid and collagen.

Therefore, development of an astaxanthin-collagen-vitamin C compound product which has high stability and is not easy to change color and can be efficiently absorbed by organisms is a research focus in the field.

Disclosure of Invention

Aiming at the defects of the prior art, the invention aims to provide the compound microcapsule powder, the preparation method and the application thereof, and the compound microcapsule powder has high product stability, high bioavailability and good antioxidation effect.

In order to achieve the aim of the invention, the invention adopts the following technical scheme:

In a first aspect, the present invention provides a compounded microcapsule powder comprising 10-20 parts (e.g., 12 parts, 14 parts, 16 parts, 18 parts, etc.) astaxanthin microcapsule powder, 100-200 parts (e.g., 120 parts, 140 parts, 160 parts, 180 parts, 200 parts, etc.) hydrolyzed collagen, and 2-7 parts (e.g., 3 parts, 4 parts, 5 parts, 6 parts, etc.) vitamin C microcapsule powder.

The astaxanthin microcapsule powder is prepared by the following method, which comprises the following steps:

(1) Pretreating astaxanthin oleoresin to obtain astaxanthin pretreatment;

(2) And dissolving the astaxanthin pretreatment in embedding mixed solution, pre-emulsifying and homogenizing to obtain emulsion, heating, stirring and spray-drying the emulsion to obtain the astaxanthin microcapsule powder.

The composite microcapsule powder provided by the invention comprises three main raw materials, astaxanthin with poor stability is pretreated and embedded to form the microcapsule powder, and the astaxanthin microcapsule powder has excellent lipid solubility and water solubility, so that the problems of easy deterioration and low bioavailability of the astaxanthin raw materials in practical application are overcome; secondly, because the collagen has the property of protein, the problems of flocculation and the like can occur under the acidic condition, and the compound use of the collagen and the vitamin C is greatly restricted.

Preferably, the astaxanthin microcapsule powder comprises, in parts by weight: 5 to 16 parts (for example, 6 parts, 8 parts, 10 parts, 12 parts, 14 parts, 16 parts, etc.), 1.5 to 2 parts (for example, 1.6 parts, 1.7 parts, 1.8 parts, 1.9 parts, etc.), 0.2 to 1.5 parts (for example, 0.4 parts, 0.6 parts, 0.8 parts, 1 part, 1.2 parts, 1.4 parts, etc.), 10 to 50 parts (for example, 12 parts, 15 parts, 20 parts, 25 parts, 30 parts, 40 parts, 45 parts, etc.), 5 to 20 parts (for example, 6 parts, 8 parts, 10 parts, 12 parts, 14 parts, 16 parts, 18 parts, etc.), and filler.

Preferably, the emulsifier is sucrose fatty acid ester.

Preferably, the co-emulsifier is a combination of phospholipids and vitamin E polyethylene glycol succinate.

Preferably, the mass ratio of the phospholipid and the vitamin E polyethylene glycol succinate is (1-5): 1, and for example, can be 2:1, 3:1, 4:1 and the like.

Preferably, the wall material is octenyl succinic acid monosarate.

Preferably, the filling material is a combination of solid corn syrup and erythritol.

Preferably, the mass ratio of the solid corn syrup to the erythritol is (0.9-1.1): (0.9-1.1), and for example, can be 0.9:1, 1:1, 1:0.9, etc.

Preferably, the pretreatment is carried out by mixing astaxanthin oleoresin with emulsifier, co-emulsifier and 1-3 parts of water and shearing.

Preferably, the shearing temperature is 8-12 ℃ (e.g. 9 ℃, 10 ℃, 11 ℃ and the like), the rotation speed is 8000-12000rpm (e.g. 9000rpm, 10000rpm, 11000rpm and the like) and the time is 15-20min (e.g. 16min, 17min, 18min, 19min and the like).

Preferably, the embedding mixture is obtained by dissolving the wall material and the filling material in water.

The shear rate of the pre-emulsification is 10000-12000rpm (for example, 10500rpm, 11000rpm, 11500rpm, etc.), and the time is 1-3min (for example, 1.5min, 2min, 2.5min, etc.).

Preferably, the pressure of the homogenization is 40-60MPa (e.g., may be 45MPa, 50MPa, 55MPa, etc.).

Preferably, the temperature of the heating and stirring is 85-95deg.C (86 ℃, 88 ℃, 90 ℃, 92 ℃, 94 ℃ etc. for example) and the time is 30-40min (32 min, 34min, 36min, 38min, etc. for example).

The invention overcomes the inherent defects of the fat-soluble astaxanthin raw material in application by using a microencapsulation technology, and solves the problems of low bioavailability, poor water solubility and the like; the combined use of the wall material, the filling material and the emulsifier greatly reduces the particle size of the astaxanthin microcapsule powder, achieves the nano-scale and improves the bioavailability.

Preferably, the hydrolyzed collagen is bovine bone-derived collagen.

Preferably, the molecular weight of the hydrolyzed collagen is 200-1000Da (e.g., 300Da, 400Da, 500Da, 600Da, 700Da, 800Da, 900Da, etc.), preferably 400-800Da.

Preferably, the vitamin C microcapsule powder comprises the following components in parts by weight: 10-20 parts (for example, 12 parts, 14 parts, 16 parts, 18 parts, etc.), 5-10 parts (for example, 6 parts, 7 parts, 8 parts, 9 parts, etc.), 0.5-1.5 parts (for example, 0.6 parts, 0.8 parts, 1 part, 1.2 parts, 1.4 parts, etc.) of stabilizer.

Preferably, the embedding wall material comprises any one or a combination of at least two of hydrogenated vegetable oil, glycerol fatty acid ester, beeswax, carnauba wax or palm oil, preferably glycerol fatty acid ester.

Preferably, the stabilizing agent comprises any one or a combination of at least two of citric acid, malic acid, tartaric acid or lactic acid, preferably citric acid.

Preferably, the vitamin C microcapsule powder is prepared by a method comprising:

(1) Mixing vitamin C with stabilizer, and pulverizing to obtain mixture powder;

(2) And mixing the mixture powder with an embedding wall material, and atomizing to obtain the vitamin C microcapsule powder.

Preferably, the particle size of the mixture powder is 100 to 350. Mu.m, for example, 120. Mu.m, 140. Mu.m, 160. Mu.m, 180. Mu.m, 200. Mu.m, 220. Mu.m, 240. Mu.m, 260. Mu.m, 280. Mu.m, 300. Mu.m, 320. Mu.m, 340. Mu.m, etc.

Preferably, the atomization pressure is 0.2-0.4MPa (for example, 0.25MPa, 0.3MPa, 0.35MPa, etc.), and the material temperature during atomization is 13-17 ℃ (for example, 14 ℃, 15 ℃, 16 ℃ and the like).

In a second aspect, the present invention provides a method for preparing the compound microcapsule powder according to the first aspect, wherein the preparation method comprises uniformly mixing astaxanthin microcapsule powder, hydrolyzed collagen and vitamin C microcapsule powder.

In a third aspect, the present invention provides the use of a formulated microcapsule powder as described in the first aspect in an oral product.

Preferably, the oral product comprises an oral cosmetic product or an oral health product.

Preferably, the dosage form of the oral product comprises a liquid dosage form or a solid dosage form.

Preferably, the mass percentage of the compound microcapsule powder in the oral product is 10% -60%, for example, 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55% and the like.

The numerical ranges recited herein include not only the recited point values, but also any point values between the recited numerical ranges that are not recited, and are limited to, and for the sake of brevity, the invention is not intended to be exhaustive of the specific point values that the recited range includes.

Compared with the prior art, the invention has the following beneficial effects:

1. the composite microcapsule powder provided by the invention comprises three main raw materials, wherein the astaxanthin microcapsule powder is excellent in both fat solubility and water solubility, and the problems that the astaxanthin raw materials are easy to deteriorate and low in bioavailability in the prior practical application are overcome; secondly, because the problems of color change, agglomeration, flocculation and the like of the collagen can occur under the acidic condition, the compound use of the collagen and the vitamin C is greatly restricted, the vitamin C is embedded to form the vitamin C microcapsule powder, the problems of color change agglomeration and the like of the two matched use are effectively overcome, the effect of the compound microcapsule powder on eliminating DPPH free radicals can be greatly improved, and the excellent antioxidation capability is reflected.

2. The astaxanthin microcapsule powder obtained by the invention has the bioavailability of 3-5 times of astaxanthin oleoresin and the DPPH free radical clearance rate of 1.88 times of astaxanthin oleoresin through Caco2 cell uptake experiments.

3. The composite microcapsule powder provided by the invention has high stability, high bioavailability and good antioxidation effect.

Drawings

FIG. 1 is a state diagram of mixture C1 of test example 2 after 20 days of accelerated test;

FIG. 2 is a state diagram of mixture C2 of test example 2 after 20 days of accelerated test;

FIG. 3 is a state diagram of mixture C3 of test example 2 after 20 days of accelerated test;

FIG. 4 is a state diagram of mixture C4 of test example 2 after 20 days of accelerated test;

FIG. 5 is a state diagram of mixture C5 of test example 2 after 20 days of accelerated test;

FIG. 6 is a state diagram of mixture C6 of test example 2 after 20 days of accelerated test.

Detailed Description

The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.

The terms "comprising," "including," "having," "containing," or any other variation thereof, are intended to cover a non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, step, method, article, or apparatus.

"Optional" or "any" means that the subsequently described event or event may or may not occur, and that the description includes both cases where the event occurs and cases where the event does not.

The indefinite articles "a" and "an" preceding an element or component of the invention are not limited to the requirement (i.e. the number of occurrences) of the element or component. Thus, the use of "a" or "an" should be interpreted as including one or at least one, and the singular reference of an element or component includes the plural reference unless the amount clearly dictates otherwise.

The description of the terms "one embodiment," "some embodiments," "exemplarily," "specific examples," or "some examples," etc., herein described means that a specific feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this document, the schematic representations of the above terms are not necessarily for the same embodiment or example.

In the present invention, percentages and percentages are by mass unless explicitly stated otherwise. Unless otherwise specified, all experimental procedures used are conventional and all materials, reagents, etc. used are commercially available.

The particle size of the invention adopts An Dongpa nanometer particle size instrument, litesize500 to measure the median particle size;

the molecular weight of the invention adopts An Dongpa nm particle diameter instrument, litesize500 to measure the molecular weight;

astaxanthin oleoresin: wherein the astaxanthin content is 13%, purchased from Dalian medical North Bio Inc.;

collagen: bovine bone source was purchased from Zhejiang core Biotechnology Co.

Preparation example 1

The preparation example provides hydrolyzed collagen, and the preparation method comprises the following steps:

(1) Adding collagen into 10 times of water for dissolution, adding hydrochloric acid in the stirring process to ensure that the acid content in the reaction liquid is 0.04%, hydrolyzing at 10 ℃ for 3 hours until the weight average molecular weight is 550Da, and neutralizing to pH 6 after the hydrolysis is completed to obtain emulsion;

b) And spray drying the emulsion to obtain the hydrolyzed collagen.

Preparation example 2

The preparation example provides a series of astaxanthin pretreatment a1-a6, the raw material composition is shown in table 1, and the preparation method is as follows: mixing astaxanthin oleoresin with emulsifier (sucrose fatty acid ester), co-emulsifier (phospholipid and vitamin E polyethylene glycol succinate TPGS) and water, and shearing at 10deg.C and 10000rpm for 15min to obtain astaxanthin pretreatment.

TABLE 1

Component (g)	a1	a2	a3	a4	a5	a6
							Astaxanthin oleoresin	10	10	10	10	10	10
Sucrose fatty acid ester	/	1.5	1.5	1.5	1.5	1.5
							TPGS	/	/	0.2	0.2	0.2	0.2
Phospholipid	/	/	/	0.2	0.2	1.0
							Water and its preparation method	/	/	/	/	1	1

Test example 1

This test example was conducted on the astaxanthin pretreatment of a1-a6 in preparation example 2 for oil solubility, water solubility and intestinal juice dissolution ratio, and the test results are shown in Table 2.

TABLE 2

According to the table data, the selection of the emulsifier and the auxiliary emulsifier is critical to the pretreatment of the astaxanthin oleoresin, and the oil solubility, the water solubility and the intestinal juice dissolution of the astaxanthin oleoresin raw material are poor; the best results are obtained by mixing the astaxanthin oleoresin material, emulsifier (sucrose fatty acid ester), co-emulsifier (phospholipid and TPGS) and water and shearing.

Preparation example 3

The preparation example provides a series of astaxanthin microcapsule powders A1-A10, and the preparation method comprises the following steps:

A1: 25g of octenyl succinic acid monosugar ester is dissolved in 50g of water, 5g of erythritol and 5g of solid corn syrup are added, stirring is carried out until the mixture is dissolved, an astaxanthin pretreatment A1 is added, 1min is sheared at 10000rpm, 50mpa homogenization is carried out, and astaxanthin emulsion is obtained, and spray drying is carried out, so that astaxanthin microcapsule powder A1 with the particle size of 35 microns is obtained.

A2: the difference from the preparation method of the astaxanthin microcapsule powder A1 is that the astaxanthin pretreatment A1 is replaced by an equivalent amount of astaxanthin pretreatment A2, and the astaxanthin microcapsule powder A2 with the particle size of 15 μm is obtained.

A3: the difference from the preparation method of the astaxanthin microcapsule powder A1 is that the astaxanthin pretreatment A1 is replaced by an equivalent amount of astaxanthin pretreatment A3, and the astaxanthin microcapsule powder A3 with the particle size of 18.2 μm is obtained.

A4: the method is different from the preparation method of the astaxanthin microcapsule powder A1 only in that the astaxanthin pretreatment A1 is replaced by an equivalent amount of astaxanthin pretreatment A4, and the astaxanthin microcapsule powder A4 with the particle size of 1.2 mu m is obtained.

A5: the preparation method is different from the preparation method of the astaxanthin microcapsule powder A1 only in that the astaxanthin pretreatment A1 is replaced by an equivalent amount of astaxanthin pretreatment A5, and the astaxanthin microcapsule powder A5 with the particle size of 900nm is obtained.

A6: the preparation method is different from the preparation method of the astaxanthin microcapsule powder A1 only in that the astaxanthin pretreatment A1 is replaced by an equivalent amount of astaxanthin pretreatment A6, and the astaxanthin microcapsule powder A6 with the particle size of 830nm is obtained.

A7: the preparation method of the astaxanthin microcapsule powder A6 is only different from that of the astaxanthin microcapsule powder A6 in that the astaxanthin microcapsule powder A is added before spray drying: stirring the emulsion at 90 ℃ for 30min to obtain astaxanthin microcapsule powder A7 with the particle size of 210nm.

A8: the preparation method of the astaxanthin microcapsule powder A7 is different from the preparation method of the astaxanthin microcapsule powder A7 only in that the octenyl succinic acid monosugar ester is replaced by the same amount of sodium starch octenyl succinate, and the astaxanthin microcapsule powder A8 with the particle size of 2.1 mu m is obtained.

A9: the preparation method of the astaxanthin microcapsule powder A9 is different from the preparation method of the astaxanthin microcapsule powder A7 only in that solid corn syrup is not added, and erythritol is adjusted to 10g, so that the astaxanthin microcapsule powder A9 with the particle size of 3.3 μm is obtained.

A10: the preparation method of the astaxanthin microcapsule powder A7 is different from the preparation method of the astaxanthin microcapsule powder A7 only in that erythritol is not added, and the solid corn syrup is adjusted to 10g, so that the astaxanthin microcapsule powder A10 with the particle size of 2.9 μm is obtained.

As can be seen from the particle size of the series of astaxanthin microcapsule powder in this preparation example, the astaxanthin microcapsule powder prepared from the astaxanthin pretreatment obtained by mixing the astaxanthin oleoresin raw material, the emulsifier (sucrose fatty acid ester), the co-emulsifier (phospholipid and TPGS) and water has smaller particle size, and the astaxanthin microcapsule powder prepared from the octenyl succinic acid monosaraboxyl ester as the wall material and the combination of the solid corn syrup and erythritol as the filling material has smaller particle size.

Preparation example 4

The preparation example provides a series of vitamin C microcapsule powders B1-B6, the raw material composition is shown in Table 3, and the preparation method is as follows: mixing vitamin C with stabilizer (citric acid), pulverizing to 200 μm, mixing the powder with embedding wall material (mono-di fatty acid ester or hydrogenated palm oil) at 60deg.C, and atomizing at 15 deg.C under 0.3MPa to obtain vitamin C microcapsule powder.

TABLE 3 Table 3

Component (g)

B1

B2

B3

B4

B5

B6

Ascorbic acid

10

Citric acid

/

1

/

1

/

Mono-di fatty acid ester

/

4.2

/

10

Hydrogenated palm oil

/

4.2

/

Test example 2

The vitamin C microcapsule powder B1-B6 provided in preparation example 4 is mixed with 200g collagen to obtain mixtures C1-C6, and the mixture is accelerated at 40deg.C for 20 days to observe the state of each mixture, as shown in figures 1-6.

As can be seen from the figure, the vitamin C and the collagen are directly mixed in the mixture C1, the stability of the mixture is poor, and discoloration and caking are easy to occur; when the vitamin C microcapsule powder is prepared from the mixture C2, C3 and C5, a stabilizer or an embedding wall material is singly added, and the stability of the obtained mixture of the vitamin C microcapsule powder and collagen is general, and the conditions of color change and caking exist; the stability of the mixture C4 and the mixture C6 is higher, the proportion of the embedded wall material added into the mixture C6 is higher, the obtained vitamin C microcapsule powder is not easy to change color after being mixed with collagen, but the content of vitamin C in the microcapsule powder is lower, the stability of the vitamin C microcapsule powder can be effectively increased by adding a small amount of stabilizer into the mixture C4, and the proportion of the vitamin C in the microcapsule powder can be ensured.

Test example 3

In vitro bioavailability assay of astaxanthin

Sample to be measured: astaxanthin oleoresin raw material (i.e. a 1), astaxanthin pretreatment a5, astaxanthin microcapsule powder A7;

The study was performed using the Caco2 cell line. Cells in the logarithmic growth phase were uniformly inoculated into 100mm cell culture dishes for subsequent cell uptake experiments. All experiments were performed using Caco2 cells within passage 20. Dissolving a sample to be tested in sterile dimethyl sulfoxide (Dimethyl sulfoxide, DMSO), mixing uniformly by vortex, and adding a drug to culture cells after the sample to be tested is diluted to the same concentration by a cell culture medium gradient; the blank group cultures cells with normal cell culture medium. After the dosing treatment, the cells were placed in a CO ₂ incubator for 1,2 and 4 hours, the cells were collected, the cells were lysed by 3mL of lysate, the astaxanthin content was measured by HPLC, and the cell uptake rate was calculated. The test results are shown in Table 4.

TABLE 4 Table 4

According to the table data, the bioavailability of the astaxanthin oleoresin raw material is lower, the bioavailability is improved after pretreatment, and when the method provided by the invention is adopted for embedding the astaxanthin, the bioavailability of the obtained astaxanthin microcapsule powder is greatly improved.

Test example 4

In vitro bioavailability assay for vitamin C

Sample to be measured: vitamin C raw material (namely B1), vitamin C microcapsule powder B4 and vitamin C microcapsule powder B6;

Caco2 cells are paved on a 12-hole transwell culture plate, after the cells grow to have cell resistance larger than 1000 omega/cm ², simulated small intestine epithelium is considered to be formed, each product with optimal concentration is given, and after the cells are treated for a certain time, samples penetrating through the cells/supernatant are collected, so that the bioavailability is deduced.

Cells in the logarithmic growth phase were uniformly inoculated into 100mm cell culture dishes for subsequent cell uptake experiments. All experiments were performed using Caco2 cells within passage 20. Dissolving a sample to be tested in sterile dimethyl sulfoxide (Dimethyl sulfoxide, DMSO), mixing uniformly by vortex, and adding a drug to culture cells after the sample to be tested is diluted to the same concentration by a cell culture medium gradient; the blank group cultures cells with normal cell culture medium. After the dosing treatment, the cells were placed in a CO ₂ incubator for 1h, the cells were collected, the lysate 3mL was used to lyse the cells, the vitamin C content was determined by HPLC, and the cell uptake rate was calculated. The test results are shown in Table 5.

TABLE 5

Sample of	Cell uptake (%)
		Vitamin C raw material B1	1.7
Vitamin C microcapsule powder B4	1.8
		Vitamin C microcapsule powder B6	2.1

According to the table data, after the vitamin C is embedded by adopting the method, the bioavailability of the obtained microcapsule powder is improved, and the cell uptake rate of B6 is higher than that of B4, but the content and the bioavailability of the vitamin C in the microcapsule powder are comprehensively considered, so that the bioavailability of the vitamin C in the vitamin C microcapsule powder B4 is higher.

Example 1

The embodiment provides a compound microcapsule powder, which comprises the following components in parts by weight: and (3) uniformly mixing 7 parts of astaxanthin microcapsule powder A, 100 parts of hydrolyzed collagen and 45 parts of vitamin C microcapsule powder B.

Example 2

The embodiment provides a compound microcapsule powder, which comprises the following components in parts by weight: and (3) uniformly mixing 7 parts of astaxanthin microcapsule powder A, 150 parts of hydrolyzed collagen and 4 7 parts of vitamin C microcapsule powder B to obtain the astaxanthin microcapsule powder.

Example 3

The embodiment provides a compound microcapsule powder, which comprises the following components in parts by weight: and (3) uniformly mixing 7 parts of astaxanthin microcapsule powder A, 200 parts of hydrolyzed collagen and 42 parts of vitamin C microcapsule powder B to obtain the astaxanthin microcapsule powder.

Test example 5

Antioxidant Capacity test

Taking 0.01g of sample to be measured, fixing the volume in a 100mL volumetric flask for standby, taking 1mL of the volumetric flask, and fixing the volume again to obtain the sample liquid to be measured. 1mL of 1X 10 ^-4 mmol/mL DPPH-ethanol solution (95%) is measured, 1mL of sample solution is added, shaking is carried out, after reaction is carried out in the dark for 40min, 95% ethanol is used as reference solution, and the absorbance Ai of the reaction system at 517nm is measured; and simultaneously measuring the absorbance Ac of 1mL of DPPH solution and the same volume of acetone solvent and the absorbance Aj of the sample solution and the same volume of acetone solvent. Calculating the clearance of the sample according to the formula:

clearance = [ Ac- (Ai-Aj) ]/ac×100%;

The test results are shown in Table 6.

TABLE 6

According to the table data, the astaxanthin microcapsule powder, the collagen and the vitamin C microcapsule powder are compounded to obtain the product with good antioxidation effect.

The applicant states that the process of the invention is illustrated by the above examples, but the invention is not limited to, i.e. does not mean that the invention must be carried out in dependence on the above process steps. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of selected raw materials, addition of auxiliary components, selection of specific modes, etc. fall within the scope of the present invention and the scope of disclosure.

The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.

In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.

Claims

1. The compound microcapsule powder is characterized by comprising 10-20 parts of astaxanthin microcapsule powder, 100-200 parts of hydrolyzed collagen and 2-7 parts of vitamin C microcapsule powder;

(1) Pretreating astaxanthin oleoresin to obtain astaxanthin pretreatment;

2. The compound microcapsule powder according to claim 1, wherein the astaxanthin microcapsule powder comprises, in parts by weight: 5-16 parts of astaxanthin oleoresin, 1.5-2 parts of emulsifier, 0.2-1.5 parts of auxiliary emulsifier, 10-50 parts of wall material and 5-20 parts of filling material.

3. The compound microcapsule powder according to claim 2, wherein the emulsifier is sucrose fatty acid ester;

preferably, the co-emulsifier is a combination of phospholipids and vitamin E polyethylene glycol succinate;

preferably, the mass ratio of the phospholipid and the vitamin E polyethylene glycol succinate is (1-5): 1.

4. A compounded microcapsule powder according to claim 2 or 3, wherein the wall material is octenyl succinic acid monosarate;

Preferably, the filling material is a combination of solid corn syrup and erythritol;

Preferably, the mass ratio of the solid corn syrup to the erythritol is (0.9-1.1): 0.9-1.1.

5. The compound microcapsule powder according to any one of claims 1-4, wherein the pretreatment method is to mix astaxanthin oleoresin with emulsifier, co-emulsifier and 1-3 parts of water and then shear;

preferably, the shearing temperature is 8-12 ℃, the rotating speed is 8000-12000rpm, and the time is 15-20min.

6. The compound microcapsule powder according to any one of claims 1 to 5, wherein the embedding mixture is obtained by dissolving a wall material and a filler material in water;

The shearing rotation speed of the pre-emulsification is 10000-12000rpm, and the time is 1-3min;

preferably, the homogenized pressure is 40-60MPa;

preferably, the temperature of the heating and stirring is 85-95 ℃ and the time is 30-40min.

7. The compound microcapsule powder according to any one of claims 1-6, wherein the hydrolyzed collagen is bovine bone-derived collagen;

Preferably, the molecular weight of the hydrolyzed collagen is 200-1000Da, preferably 400-800Da.

8. The compound microcapsule powder according to any one of claims 1 to 7, wherein the vitamin C microcapsule powder comprises, in parts by weight: 10-20 parts of vitamin C, 5-10 parts of embedding wall material and 0.5-1.5 parts of stabilizer;

Preferably, the embedding wall material comprises any one or a combination of at least two of hydrogenated vegetable oil, glycerin fatty acid ester, beeswax, carnauba wax or palm oil, preferably glycerin fatty acid ester;

Preferably, the stabilizing agent comprises any one or a combination of at least two of citric acid, malic acid, tartaric acid or lactic acid, preferably citric acid;

(1) Mixing vitamin C with stabilizer, and pulverizing to obtain mixture powder;

(2) Mixing the mixture powder with an embedding wall material, and atomizing to obtain vitamin C microcapsule powder;

Preferably, the particle size of the mixture powder is 100-350 μm;

preferably, the atomization pressure is 0.2-0.4MPa, and the temperature of the material during atomization is 13-17 ℃.

9. A method for preparing the compound microcapsule powder according to any one of claims 1-8, comprising uniformly mixing astaxanthin microcapsule powder, hydrolyzed collagen and vitamin C microcapsule powder.

10. Use of the compounded microcapsule powder of any of claims 1-8 in an oral product;

Preferably, the oral product comprises an oral cosmetic product or an oral healthcare product;

Preferably, the dosage form of the oral product comprises a liquid dosage form or a solid dosage form;

preferably, the mass percentage of the compound microcapsule powder in the oral product is 10% -60%.